WO2016032733A2 - Procédé de chargement de parfum dans un aérogel et aérogel imprégné de parfum basé sur des substances de qualité alimentaire - Google Patents

Procédé de chargement de parfum dans un aérogel et aérogel imprégné de parfum basé sur des substances de qualité alimentaire Download PDF

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Publication number
WO2016032733A2
WO2016032733A2 PCT/US2015/044474 US2015044474W WO2016032733A2 WO 2016032733 A2 WO2016032733 A2 WO 2016032733A2 US 2015044474 W US2015044474 W US 2015044474W WO 2016032733 A2 WO2016032733 A2 WO 2016032733A2
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WIPO (PCT)
Prior art keywords
aerogel
food grade
flavor
protein isolate
loading
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PCT/US2015/044474
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English (en)
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WO2016032733A3 (fr
Inventor
Cuie Yan
Peter S. Given, Jr.
Gary Huvard
Rajendar Reddy MALLEPALLY
Mark A. Mchugh
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Pepsico , Inc.
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Application filed by Pepsico , Inc. filed Critical Pepsico , Inc.
Priority to EP15835352.4A priority Critical patent/EP3185699A2/fr
Publication of WO2016032733A2 publication Critical patent/WO2016032733A2/fr
Publication of WO2016032733A3 publication Critical patent/WO2016032733A3/fr

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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/212—Starch; Modified starch; Starch derivatives, e.g. esters or ethers
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231—Pectin; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/256—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/275—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of animal origin, e.g. chitin
    • A23L29/281—Proteins, e.g. gelatin or collagen

Definitions

  • the present invention relates to a method of preparing food grade aerogels, and a method for the loading of flavor into a prepared food grade aerogel, in which the flavor is loaded, and the resulting food grade aerogel.
  • Flavors are important in any food formula and can influence the finished product quality and cost. It is important to harness flavors and aromas to make products appealing to consumers for as long as possible after the product is initially produced.
  • the complex systems associated with flavors are often difficult and expensive to control, because one flavor may contain thousands of flavor compounds, and most of the flavor compounds are delicate and volatile, particularly top notes. They escape and are oxidized quickly and easily at or below room temperature in the atmosphere. Thus, their retention and integrity are big concerns for food manufacturers.
  • the present invention pertains to the formation of food grade aerogels from one or more food grade materials; and the impregnation of flavors onto the aerogels assisted by supercritical carbon dioxide technology.
  • a food grade hydrogel is formed, followed by aerogel formation through an alcogel.
  • flavor is impregnated onto the aerogel assisted by supercritical carbon dioxide.
  • the flavor loaded food grade aerogel releases flavors loaded therein under certain triggers, such as pH, ion strength, moisture, temperature, or mechanic force. Aerogel formation is performed with a series of suspensions in gradually increasing ethanol concentrations before overnight suspension in 100% ethanol solution.
  • Supercritical carbon dioxide technology is used for both formation of the aerogel and for impregnating of the formed aerogel with a flavor.
  • Resulting food grade aerogels possess a high flavor loading capacity of up to about 70%, which is well above the average loading capacity of the most common flavor encapsulation technology via spray drying (which are up to 20% capacity loading), while maintain the integrity of flavors, particularly top notes.
  • Figure 1 a is a scanning electron microscopy image of an alginate aerogel prepared for flavor loading as described herein.
  • Figure lb is a scanning electron microscopy image of a starch aerogel prepared for flavor loading as described herein.
  • Figure lc is a scanning electron microscopy image of a pectin aerogel prepared for flavor loading as described herein.
  • Figure 2 depicts a sample drawing of equipment used to perform flavor loading steps as described herein.
  • Figures 3a and 3b are thermogravimetril analysis of limonene flavor retention of three different polysaccharide aerogels prepared by the methods described herein.
  • Figures 4a and 4b are graphical representations displaying thermogravimetric analysis of S1O2 aerogel loaded with limonene.
  • Figure 5 is a graphical representation demonstrating the shelf-life of a limonene loaded S1O2 aerogel.
  • Aerogels are formed by removing liquid from a gel, for example, evaporating water from a hydrogel. Aerogels are porous and lightweight materials, with high porosity, low density, and a large surface area. Typically, aerogels are formed from inorganic compounds such as silica. More recently, the concept of polysaccharides from plants, alga and crustaceans as aerogel-forming materials has emerged. However, to date, food applications of food grade aerogels do not exist. The present disclosure sets forth a method of applying food grade aerogels from a number of sources, including those not yet considered, to the realm of flavor loading and encapsulations.
  • a first aspect of the present disclosure thus relates generally to a method of embedding flavors witin highly porous food grade aerogels through a sub or super critical carbon dioxide assisted process.
  • the method comprises the steps of selecting a food grade material for preparation of a porous food grade aerogel, wherein said food grade material is a non-silica organic material and wherein the food grade aerogel provides for release of a flavor loaded therein; preparing the food grade aerogel using a supercritical carbon dioxide assisted process; and impregnating the food grade aerogel with flavor using a supercritical carbon dioxide assisted process, thereby forming a flavor loaded food grade aerogel, from which loaded flavors can ultimately be released.
  • the food grade aerogel disclosed herein may be prepared from a good grade material selected from a polysaccharide, protein, solid lipid, or a combination thereof. Resulting aerogels are not only stable, similar to inorganic aerogels, but also safe to ingest. Using the method described herein an aerogel is successfully loaded with flavor, and the resulting flavors are able to retain both their nonvolatile and volatile components at very high loading levels while maintaining their integrity until the release is desired. Encapsulation is the technique by which one material or a mixture of materials (known as active or core material) is coated with or entrapped within another material or system (referred to as shell, wall material, matrix, carrier or encapsulant). In one embodiment, the flavor may be entrapped within the aerogel porous structure.
  • the flavor may be coated on the interface of the food grade aerogel porous structure.
  • the actual entrapment mechanism will depend in part on the resulting pore size of the food grade aerogel, the material selected for creating the aerogel, and/or the nature of the flavor compounds.
  • the step of selecting a food grade material for preparing the porous food grade aerogel may comprise selection of one or more of: starch, pectin, alginate, cellulose, starch sodium octenyl succinate, locust bean gum, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, whey protein isolate, soy protein isolate, pea protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the step of selecting a food grade materal for preparing the porous food grade aerogel may comprise selection of two or more of: starch, pectin, alginate, cellulose, starch sodium octenyl succinate, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, whey protein isolate, soy protein isolate, pea protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the step of selecting a food grade materal for preparing the porous food grade aerogel may comprise selection of three or more of: starch, pectin, alginate, cellulose, starch sodium octenyl succinate, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, whey protein isolate, soy protein isolate, pea protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • Starch is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Starch consists of two major components, amylose and amylopectin.
  • Amylose is linearly comprise of a-(l ⁇ 4)-linked D-glucopyranosyl units with an average molecular weight of 500 kg/mol. Amylose forms the amorphous part of starch, while amylopectin is the component of the crystalline parts. Amylopectin comprises a backbone of cc-(l ⁇ 4)-linked D-glucopyranosyl units, with branching taking place with a(l ⁇ 6) bonds occurring every 24 to 30 glucose units.
  • Suitable starch for preparation of the aerogels described herein can be obtained from any number of commercial sources.
  • Pectin is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Pectin is a grouping of acid structural polysaccharides found in fruit and vegetables and is prepared mainly from citrus peel waste and apple pomace. Suitable pectin for preparation of the aerogels described herein can be obtained from any number of commercial sources.
  • Alginate is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Alginate also known as alginic acid sodium salt, is a natural anionic polysaccharide mainly derived from brown algae. It is a linear random copolymer of (l,4')-linked ⁇ -D-mannuronic acid and -L-guluronic acid monomers with the chemical structure.
  • Alginates are natural polyelectrolytes that form hydrogels at low concentrations (1- 2%). Gelling of alginates occurs when di or trivalent cations participate in the interchain binding between sequences of mannuronic and guluronic acid residues.
  • Cellulose is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Cellulose is an organic polysaccharide having a linear structure comprise of ⁇ -(1 ⁇ 4) linked D-glucopyranosyl units. It is an important structural component of the cell wall of green plants and many forms of algae. It is the most abundant
  • polysaccharide on earth and suitable sources for the preparation of the aerogel described herein is readily available from any number of commercial sources.
  • Starch sodium octenyl succinate is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Starch sodium octenyl succinate is a chemically modified starch that results during the reaction of starch with succinic acid and octanol.
  • Suitable alginate for preparation of the aerogel described herein can be obtained from any number of commercial sources.
  • Locust bean gum is a suitable food grade material for preparing the porous food grade aerogel described herein and can be found from any number of commercial sources.
  • Carrageenan is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Carrageenans or carrageenins are a family of linear sulphated polysaccharides that are extracted from red edible seaweeds.
  • Carrogeenan is another algae- derived polysaccharide that shows gelling capacity induced by cations.
  • Suitable carrageenans for preparation of the aerogel described herein can be obtained from any number of commercial sources.
  • Agar is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Agar is a polymer made up of subunits of galactose and is a component of algae cell walls.
  • Suitable agar for preparation of the aerogel described herein can be obtained from commercial sources such as AGAR RS-100TM from TIC Gums (Belcamp, MD).
  • Xanthum gum is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Xanthum gum is a natural gum polysaccharide used as a food additive and rheology modifier. It is produced by a biotechnological process involving fermentation of glucose or sucrose by Xanthomonas campestris. It is capable of producing a large increase in viscosity by adding a very small quantity of bum, on the order of one percent. In most foods, it is used at a percentage of about 0.5%, or as low as 0.05%.
  • Xantham gum is very stable under a wide range of temperatures and pH and is readily available from any number of commercial sources.
  • Guar gum is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Guar gum is a galactomannan, which are polysaccharides consisting of a mannose backbone with galactose side groups ((l-4)-linked B-D- mannopyranose backbone with branchpoints from their 6-positions linked to cc-D-galactose, i.e. 1-6-linked cc-D-galactopyranose).
  • Galactomannans are commonly used in foods as stabilizers and guar gum may be used in ice cream to reduce melting.
  • Suitable guar gum for preparing the aerogel described herein may be found at any number of commercial sources.
  • Chitosan is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Chitosan is a linear polysaccharide composed of randomly distributed -(l-4)-linked D-glucosamine (deacetylated unit) and N-acetyl-D-glucosamine (acetylated unit). It is made by treating shrimp and other crustacean shells with the alkali sodium hydroxide.
  • Gelatin is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Gelatin is an irreversibly hydrolyzed form of collagen often derived from the bones, skin, and cartilage of fish, swing, and/or cattle. It is commonly used as a gelling agent in foods and may be obtained from any number of commercial sources.
  • Casein is a suitable food grade material for preparing the porous food grade aerogel described herein and can be found from any number of commercial sources.
  • Whey protein isolate WPI is a suitable food grade material for preparing the porous food grade aerogel described herein. WPI comes from whey protein and container greater than 90% protein. As used herein, WPI specifically excludes whey protein concentrate. Because whey protein concentrate comprises a lower protein content, use of whey protein concentrate would result in a pore size too large to be referred to as an aerogel. WPI is a collection of globular proteins that is isolated from whey, a by-product of cheese manufactured from bovine milk.
  • WPI can be commercially obtained from sources such as NZMP ALACEN 895TM from Nealanders International Inc. (Rocky River, OH), or WPI BiPro with a protein content of 94% w/w from Davisco Foods.
  • Soy protein isolate is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • SPI is a highly refined or purified form of soy protein with a minimum protein content of about 90% on a dry basis. It is made from defatted soy flour, which has had most of the non-protein components, fats and carbohydrates removed. It can be obtained from commercial sources such as PRO FAM781TM from ADM Protein Specialties Division (Decatur, IL).
  • SPI specifically excludes soy protein concentrate. Again, soy protein concentration would not result in aerogel formation.
  • Pea protein isolate is a suitable food grade material for preparing the porous food grade aerogel described herein. It is a natural vegetable protein and provides a number of nutritional benefits. PPI can be obtained from any variety of species of pea and is specifically meant to be exclusive of pea protein concentrate. As used herein, pea protein isolate specifically excludes pea protein concentrate, which is not suitable for formation of an aerogel due to its low protein concentration.
  • Potato protein isolate is a suitable food grade material for preparing the porous food grade aerogel described herein. Potato protein isolate can be obtained from any varietiy of potatoes and is specifically meant to exclude pea protein concentrate. PoPI, as used herein, is specifically meant to exclude potato protein concentrate, which is not suitable for formation of an aerogel due to its low protein concentration.
  • Zein is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Zein is an insoluble cereal prolamine proteins. It is clear, odorless, tasteless, hard, water-insoluble and edible. Zein provides an excellent water barrier, offering extended shelf-life, particularly under high-humidity, and high heat conditions.
  • zein provides for flavor encapsulations with very high flavor load concentration and retention not yet seen in the art. Commercially available zein can be obtained from any number of sources.
  • Lecithin is a suitable food grade material for preparing the porous food grade aerogel described herein. It is an all-natural emulsifier derived from product such as soy, eggs, sunflower and canola seeds. Lecithins are readily commercial available from a number of sources.
  • Stearic acid is a suitable food grade material for preparing the porous food grade aerogel described herein. It is a saturated fatty acid that occurs in many animal and vegetable fats and oils.
  • Beeswax is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Beeswax is a natural wax produced in the bee hive of honey bees of the genus Apis.
  • Cottonseed wax is a suitable food grade material for preparing the porous food grade aerogel described herein.
  • Cottonseed wax is a wax made from hydrogenated cottonseed oil.
  • Carnauba wax is a suitable food grade material for preparing the porous food grade aerogel described herein. It is a wax from the leaves of the carnauba palm Copernicia prunifera. These waxes are readily obtainable from any number of commercial sources.
  • Palm oil is an edible vegetable oil derived from the mesocarp of the fruit of the oil palms.
  • Palm kernel oil is an edible plant oil derived from the kernel of the oil palm. Both oils are readily obtainable from any number of commercial sources.
  • the food grade material for preparation of the aerogel may comprise gelatin together with one or more of: pectin, alginate, cellulose, starch sodium octenyl succinate, locust bean gum, carrageenan, agar, xanthan gum, guar gum, chitosan, casein, whey protein isolate, soy protein isolate, pea protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the food grade material for preparation of the aerogel may comprise pectin together with one or more of: starch, alginate, cellulose, starch sodium octenyl succinate, locust bean gum, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, whey protein isolate, soy protein isolate, pea protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the food grade material for preparation of the aerogel may comprise alginate together with one or more of: starch, pectin, cellulose, starch sodium octenyl succinate, locust bean gum, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, whey protein isolate, soy protein isolate, pea protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the food grade material for preparation of the aerogel may comprise cellulose together with one or more of: starch, pectin, alginate, starch sodium octenyl succinate, locust bean gum, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, whey protein isolate, soy protein isolate, pea protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the food grade material for preparation of the aerogel may comprise cellulose together with chitosan, gelatin, and solid lipids.
  • the food grade material selected is a combination of cellulose and chitosan.
  • the food grade material selected is a combination of cellulose and gelatin.
  • the food grade material selected is a combination of alginate with gelatin. In one embodiment, the food grade material selected is a combination of alginate with chitosan.
  • the food grade material for preparation of the aerogel may comprise whey protein isolate together with one or more of: starch, pectin, alginate, cellulose, starch sodium octenyl succinate, locust bean gum, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, soy protein isolate, pea protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the food grade material for preparation of the aerogel may comprise soy protein isolate together with one or more of: starch, pectin, alginate, cellulose, starch sodium octenyl succinate, locust bean gum, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, whey protein isolate, pea protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the food grade material for preparation of the aerogel may comprise pea protein isolate together with one or more of: starch, pectin, alginate, cellulose, starch sodium octenyl succinate, locust bean gum, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, whey protein isolate, soy protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the food grade material for preparation of the aerogel may comprise potato protein isolate together with one or more of: starch, pectin, alginate, cellulose, starch sodium octenyl succinate, locust bean gum, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, whey protein isolate, soy protein isolate, pea protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the food grade material for preparation of the aerogel may comprise zein together with one or more of: starch, pectin, alginate, cellulose, starch sodium octenyl succinate, locust bean gum, carrageenan, agar, xanthan gum, guar gum, chitosan, gelatin, casein, whey protein isolate, soy protein isolate, pea protein isolate, potato protein isolate, zein, lecithins, stearic acid, beeswax, cottonseed wax, carnauba wax, milk fat, palm and palm kernel oil, or any combination thereof.
  • the food grade material for preparation of the aerogel may comprise whey protein isolate together with pectin. In one embodiment, the food grade material for preparation of the aerogel may comprise whey protein isolate together with alginate. In one embodiment, the food grade material for preparation of the aerogel may comprise whey protein isolate together with carrageenan. In one embodiment, the food grade material for preparation of the aerogel may comprise whey protein isolate together with one of: pectin, alginate, locust bean gum, or carrageenan and zein.
  • the food grade material for preparation of the aerogel may comprise whey protein isolate together with one of: pectin, alginate, locust bean gum or carrageenan; zein; and with one of: beeswax, cottonseed wax, or carnauba wax.
  • the food grade material for preparation of the aerogel may comprise soy protein isolate together with pectin. In one embodiment, the food grade material for preparation of the aerogel may comprise soy protein isolate together with alginate. In one embodiment, the food grade material for preparation of the aerogel may comprise soy protein isolate together with carrageenan. In one embodiment, the food grade material for preparation of the aerogel may comprise soy protein isolate together with one of: pectin, alginate, locust bean gum or carrageenan and zein.
  • the food grade material for preparation of the aerogel may comprise soy protein isolate together with one of: pectin, alginate, locust bean gum or carrageenan; zein; and with one of: beeswax, cottonseed wax, or carnauba wax.
  • the food grade material for preparation of the aerogel may comprise pea protein isolate together with pectin. In one embodiment, the food grade material for preparation of the aerogel may comprise pea protein isolate together with alginate. In one embodiment, the food grade material for preparation of the aerogel may comprise pea protein isolate together with carrageenan. In one embodiment, the food grade material for preparation of the aerogel may comprise pea protein isolate together with one of: pectin, alginate, locust bean gum or carrageenan and zein.
  • the food grade material for preparation of the aerogel may comprise pea protein isolate together with one of: pectin, alginate, locust bean gum or carrageenan; zein; and with one of: beeswax, cottonseed wax, or carnauba wax.
  • the food grade material for preparation of the aerogel may comprise potato protein isolate together with pectin. In one embodiment, the food grade material for preparation of the aerogel may comprise potato protein isolate together with alginate. In one embodiment, the food grade material for preparation of the aerogel may comprise potato protein isolate together with carrageenan. In one embodiment, the food grade material for preparation of the aerogel may comprise potato protein isolate together with one of: pectin, alginate, locust bean gum or carrageenan and zein.
  • the food grade material for preparation of the aerogel may comprise potato protein isolate together with one of: pectin, alginate, locust bean gum or carrageenan; zein; and with one of: beeswax, cottonseed wax, or carnauba wax.
  • the food grade material for preparation of the aerogel may comprise stearic acid together with beeswax. In one embodiment, the food grade material for preparation of the aerogel may comprise stearic acid together with cottonseed wax. In one embodiment, the food grade material for preparation of the aerogel may comprise stearic acid together with carnauba wax.
  • Preparation of the aerogel with the selected food grade material is performed using sol-gel chemistry combined with supercritical fluid technology.
  • Gelation refers to the linking of macromolecular chains that progressively leads to larger branched yet soluble polymers, dependent on the starting material structure and conformation.
  • the term "sol” refers to the mixture of the polydisperse soluble branched polymer. As the linking process continues, the size of the branched polymer increases and its solubility decreases.
  • This polymer is permeated with finite branched polymers and is referred to as the "gel.”
  • the transition from a system with finite branched polymer to infinite molecules is referred to as the “sol-gel transition” or “gelation.”
  • Gelation can take place either by physical linking, known as physical gelation, or by chemical linking, known as chemical gelation.
  • a wet gel is first formed from the selected food grade material, followed generally by a drying of the hydrogel to form the food grade aerogel.
  • Formation of a hydrogel may involve preparation of an aqueous solution of the selected food grade material and crosslinking hydrophilic polymers.
  • a formed hydrogel should be strong enough that it will not collapse under pressure. Typically, the higher the gelatin bloom number, the better. Gelatin bloom numbers of 200-250 bloom are suitable; however, lower bloom gelatin can be cross-linked to increase the strength if necessary to achieve a suitable hydrogel.
  • the preparing of the food grade aerogel comprises formation into alcogel using ethanol and drying of the alcogel by supercritical CO2 technology. More specifically, the preparing of the food grade aerogel through alcogel comprises dehydration of a hydrogel by suspension in a series of ethanol-water solutions of increasing ethanol concentrations.
  • the formation into an alcogel happens gradually or in stages wherein dehydration of hydrogel to form alcogel comprises suspensions in each of ethanol concentrations of 20%, 40%, 60%, 80% (v/v%)) for at least 15 minutes (each solution), followed by overnight suspension (about 12 hours) in 100% ethanol solution. Progressive suspension periods in increasing ethanol concentration solutions are necessary to replace water gradually and keep the highly porous structure.
  • Drying of the alcogel by supercritical carbon dioxide generally takes place at a temperature of about 10-50°C and a pressure of about 500-5,000 psi, with the pressure depending upon the temperature used.
  • the drying step temperature for preparing the food grade aerogel is about 30 °C to about 40 °C.
  • the drying step for preparing the food grade aerogel is performed at a pressure of between 500 to about 4,000 psi.
  • the drying step for preparing the food grade aerogel is performed at a pressure of between 1,000 to about 2,500 psi.
  • the drying step for preparing the food grade aerogel is performed at a pressure of about 1,500 psi.
  • the preparing step may be performed for about 60-300 minutes. In some embodiments, the preparing step under the provided pressure and temperature conditions may take place for about 3-4 hours.
  • Resulting food grade aerogels are highly porous, with pore sizes ranging from about 1 nm to about 200 nm.
  • food grade polysaccharide aerogels comprise pore sizes ranging from about 2 to about 100 nm.
  • food grade aerogels as described herein comprise pore sizes ranging from about 2 to 50 nm.
  • food grade polysaccharide aerogels comprise a surface area of about 100 to about 700 m 2 /g.
  • the food grade polysaccharide aerogel comprises pore volumes of about 0.1 to about 3 cc/g.
  • Figures la-c depicts close up views of prepared alginate, starch, and pectin aerogels, respectively. Table 1, below, provides the typical characteristics determined for these example aerogels.
  • the method then comprises a second step of using a supercritical carbon dioxide assisted process.
  • a high pressure vessel such as Parr instruments, bench top model 5500 with magnetic stirrer drive 20 into which a flavor 10 is loaded, is used. Any flavor sufficiently soluble in carbon dioxide may be used.
  • Example flavor compounds successfully created using the method described herein include, for example, limonene, citral, ethyl butyrate, and isoamyl acetate, and their combinations.
  • a flavor 10 is loaded into the high pressure vessel 35. Flavor may be in gas, solid or liquid. In one embodiment, the flavor is in gas form.
  • the flavor is in solid form. In one embodiment, the flavor is in liquid form.
  • the food grade aerogel 5 is placed in the high pressure vessel and the vessel is then pressurized with carbon dioxide 25 for between about 10 to about 90 minutes, depending on the size of the production scale and/or the strength of the aerogel as well as the nature of the flavor (i.e., the flavor solubility with carbon dioxide).
  • the vessel is pressured for between 30-60 minutes. The vessel is then slowly depressurized to atmospheric pressure, wherein slowly means a period of time of about 30 to about 60 minutes, or no less than about 30 minutes.
  • the mixing vessel 35 may be heated with the aid of a heater jacket 30 around the vessel for flavor compounds with high vaporization temperatures, followed by use of an ice bath 15 to condense them before venting. It should be noted that the steps for flavor loading mentioned above should be sequential and must occur without any intervening steps.
  • the resulting impregnated aerogels comprise a flavor loading level of up to about 70% while maintaining 100% of their integrity but in any case, a loading level greater than 20%, which is well above the average loading level of currently available commercial products, which is up to 20%. Regarding the average load currently known, higher loading level may be possible but you would not retain the volatiles as they escape into the vent.
  • the food grade aerogel flavor encapsulation comprises a flavor loading level of between about 50 to about 60%. During experimental runs, a retention rate of 100% was shown after 2.5 months.
  • the carbon dioxide assisted flavor impregnation process described herein provides for an oxygen-free closed system under low temperature (i.e., 25 degrees C).
  • Figures 4a and 4b depict analysis of commercially available S1O2 aerogels loaded with limonene: limonene AEROSIL® 300 (D) (a hydrophilic fumed silica with a specific surface area of 300 m 2 /g), limonene silica aerogel (E), and limonene silicon dioxide nano particles (F).
  • Table 3 depicts the limonene loading possible when using these three commercially available silicon dioxide materials: D-AEROSIL® 300 ; E- a silica aerogel; and F-silicon dioxide nano particles.
  • FIG 3 and 4 clearly show that the flavor loading level of the three polysaccharide aerogels is much higher than that of the currently available S1O2 aerogel (E), nanoparticles (F) or aerosol (D).
  • Figure 5 depicts loaded limonene loss with storage time at room temperature and more specifically, the shelf-life of three limonene loaded silicon dioxide formulations: D- AEROSIL® 300; E- a silica aerogel; and F-silicon dioxide nano particles.
  • Silica aerogel lost 9% of the loaded limonene in 53 days, while there is no limonene loss of the three polysaccharide aerogels after 75 days storage as shown in Table 2.
  • Whey protein isolate (WPI) with a protein content of 94% w/w was obtained from Davisco Foods International Inc. (Le Sueur, MN) and used to prepare a stock protein solution by dissolving the WPI powder in deionized water. The solution was kept at 4°C for at least 12 hours to allow for complete dehydration of water. Hydrochloric acid and sodium hydroxide were used to adjust the pH value of the stock protein solution.
  • Example 2 Flavor Loaded Alginate Aerogel
  • the hydrogel beads were suspended in a series of ethanol-water solutions of increasing ethanol concentrations (20, 40, 60, 80 (v/v%)) for 15 minutes in each solution, followed by overnight suspension (about 12 hours) in 100% ethanol solution.
  • the alcogel beads were subsequently dried using supercritical carbon dioxide at 40°C and 1,400 psi by continuously flowing carbon dioxide through the beads at a rate of 3.5 L (STP)/min for 2 hours.
  • STP 3.5 L
  • One gram of the obtained alginate aerogel was placed in the middle of a high pressure vessel and limonene flavor oil was placed at the bottom. The vessel was pressurized with carbon dioxide to 1,000 psi. Using an externally mounted heating band, the temperature was maintained about 25°C.
  • Vigorous mixing was performed over the course of 30 to 120 minutes in various test runs under pressurized condition and then slowly depressurized over a period of 30 minutes.
  • Flavor loading amount was determined gravimetrically by aerogel weight gain, which measured weights as 1.58 grams thus, the limonene flavor loading amount could be calculated to be about 58%.
  • the limonene flavor loaded alginate aerogel were stored at 22°C in a tightly screwed capped glass bottle. After 2.5 months of storage, the limonene loading obtained gravimetrically was about 63%.
  • the solution was then transferred to plastic syringe molds and the formed gel was aged for approximately 24 hours at ambient conditions.
  • Approximately 5 to 6 cm long cylindrical hydrogels were cut into 0.5 to 0.6 cm thick discs with a razor and the discs were suspended in a series of ethanol-water solutions of increasing ethanol concentration (20, 40, 60, 80 v/v%) for 30 minutes in each solution, followed by overnight suspension in 100 % ethanol solution.
  • the alcogel discs were subsequently dried using supercritical carbon dioxide at 40 °C and 1,400 psig by continuously flowing carbon dioxide through the discs at a rate of 3.5 L (STP)/min for four hours.
  • Example 2 the high pressure vessel referenced in Example 1 was used for limonene flavor impregnation.
  • the obtained pectin aerogel was placed in the middle of the vessel and limonene flavor oil was placed at the bottom.
  • the vessel was thereafter pressurized with carbon dioxide to 1,000 psi. Using an externally mounted heating band, the temperature was maintained about 25°C. Vigorous mixing was performed over the course of 30 to 120 minutes in various test runs under pressurized condition and then slowly depressurized over a period of 30 minutes.
  • Limonene flavor loading amount was determined gravimetrically by aerogel weight gain, which measured weights as 1.4 grams; thus, the limonene flavor loading amount could be calculated to be about 40%.
  • the limonene flavor loaded pectin aerogel were stored at 22°C in a tightly screwed capped glass bottle. After 2.5 months of storage, the limonene loading obtained gravimetrically was about 25%.
  • Starch was dispersed in distilled water (10 wt%) and the dispersion was heated to 95°C with continuous stirring. A translucent solution of starch in distilled water was obtained in approximately 15 minutes. The heating was turned off and the solution was cooled to room temperature by storing at ambient conditions. The solution was then transferred to a plastic syringe and covered with parafilm. The solution gelled in
  • the gels were aged/cured overnight (about 12 hours), by placing in the refrigerator (2-8°C). Approximately 5 to 6 cm long cylindrical hydrogels were cut into 0.5 to 0.6 cm thick discs with a razor and the discs were suspended in a series of ethanol-water solutions of increasing ethanol concentration (20, 40, 60, 80 v/v%) for 30 minutes in each solution, followed by overnight suspension in 100 % ethanol solution. The alcogel discs were subsequently dried using supercritical carbon dioxide at 40 °C and 1,400 psig by continuously flowing carbon dioxide through the discs at a rate of 3.5 L (STP)/min for four hours. Then, the high pressure vessel referenced in Example 1 was used for limonene flavor impregnation.
  • limonene flavor oil was placed at the bottom.
  • the vessel was thereafter pressurized with carbon dioxide to 1,000 psi. Using an externally mounted heating band, the temperature was maintained about 25 °C. Vigorous mixing was performed over the course of 30 to 120 minutes in various test runs under pressurized condition and then slowly depressurized over a period of 30 minutes.
  • Limonene flavor loading amount was determined gravimetrically by aerogel weight gain, which measured weights as 1.55 grams; thus, the limonene flavor loading amount could be calculated to be about 55%.
  • the limonene flavor loaded starch aerogel were stored at 22°C in a tightly screwed capped glass bottle. After 2.5 months of storage, the limonene loading obtained gravimetrically was determined to be substantially the same at 55%.

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Abstract

Cette invention concerne des aérogels de qualité alimentaire qui sont utilisés pour imprégner un parfum à l'aide de la technologie du dioxyde de carbone supercritique. Une ou plusieurs substances de qualité alimentaire sont utilisées pour former l'aérogel de qualité alimentaire. La technologie du dioxyde de carbone supercritique est utilisée à la fois pour former l'aérogel et pour imprégner l'aérogel formé d'un parfum. Les aérogels de qualité alimentaire obtenus présentent une capacité de charge aromatique élevée allant jusqu'à environ 70 %, qui est très supérieure à la capacité de charge moyenne de la technique d'encapsulation de parfum la plus courante par séchage par atomisation (qui est d'environ 20 %), tout en conservant l'intégrité des parfums, en particulier des notes de tête.
PCT/US2015/044474 2014-08-26 2015-08-10 Procédé de chargement de parfum dans un aérogel et aérogel imprégné de parfum basé sur des substances de qualité alimentaire WO2016032733A2 (fr)

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WO2023170134A1 (fr) 2022-03-08 2023-09-14 Aerogel-It Gmbh Procédé de production de matériaux poreux

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WO2018138607A1 (fr) * 2017-01-24 2018-08-02 Nestec Sa Compositions comprenant des anticorps anti-fel d1 et procédés de réduction d'au moins un symptôme d'allergie humaine aux chats
CN107459588B (zh) * 2017-09-29 2019-08-27 渤海大学 一种超临界co2流体萃取技术提取荔枝草多糖的方法
CN108031448A (zh) * 2017-12-27 2018-05-15 西北师范大学 一种玉米蛋白基多孔疏水吸油材料的制备方法
CN109046190B (zh) * 2018-09-27 2021-11-26 广东工业大学 一种果胶复合二氧化硅气凝胶及其制备方法与应用
CN109876771B (zh) * 2019-04-17 2021-11-30 上海工程技术大学 一种丝瓜活性炭气凝胶材料、其制备方法和应用
US20220304316A1 (en) * 2021-03-26 2022-09-29 Spellbound Development Group, Inc. Systems and methods for flavoring and lubricating food items and cooking surfaces
US20220304350A1 (en) * 2021-03-26 2022-09-29 Spellbound Development Group, Inc. Systems and methods for imparting flavoring and/or lubrication to a surface
CN114105119B (zh) * 2021-11-26 2023-07-21 桂林电子科技大学 一种超弹性瓜尔胶碳气凝胶及其制备方法和应用
CN114958480A (zh) * 2022-05-13 2022-08-30 中国科学技术大学先进技术研究院 一种气凝胶基缓释香精的制备方法

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IT201800003239A1 (it) * 2018-03-02 2019-09-02 Materias S R L Processo per preparare un aerogelo superassorbente
WO2019167013A1 (fr) * 2018-03-02 2019-09-06 Materias S.R.L. Procédé de préparation d'un aérogel superabsorbant
WO2023170134A1 (fr) 2022-03-08 2023-09-14 Aerogel-It Gmbh Procédé de production de matériaux poreux

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